CN103396295B - A kind of method extracting resveratrol ingredient from giant knotweed - Google Patents
A kind of method extracting resveratrol ingredient from giant knotweed Download PDFInfo
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Abstract
The invention provides a kind of method extracting resveratrol ingredient from giant knotweed, adopt the raw material handled well through enzymatic hydrolysis and fermentation, can be giant knotweed, peanut rhizome, grape the plant such as branches and leaves, mulberry leaf as raw material.The alcohol solvent adding 80% concentration after re-adding superoxide-dismutase according to raw material ratio carries out extracting, extracting solution merges the concentrated and complete receipts ethanol of final vacuum, concentrated solution adds chitosan saturated solution, extract is separated out in the mode of precipitation, the alcohol solvent adding 20 times of precipitate weight 40% precipitate is dissolved and filter, filtered liquid concentrated after add chitosan solution, leave standstill the precipitate that centrifugation obtains solid under normal temperature.The alcohol solvent again adding 20 times of precipitate weight 40% precipitate is dissolved and filter, filtered liquid concentrated after add chitosan solution, the precipitate that centrifugation obtains solid is left standstill under normal temperature, pure water washing, under washings non-pigment composition state, pulverizes the product both obtaining 50%-65% after vacuum-drying; It can improve yield more than 30% compared with existing production method.
Description
One, technical field
The present invention relates to a kind of method extracting resveratrol ingredient from giant knotweed.Also be applicable to from peanut rhizome, the branches and leaves of grape, the plants such as mulberry leaf extract trans-resveratrol as raw material.Belong to biological technical field.
Two, background technology
Trans-resveratrol is a kind of natural antioxidant; the viscosity of blood can be reduced; suppress hematoblastic improper condensation; prevention impatient hard plug, cerebral embolism, hepar damnification; provide protection and arterial vascular diastole is had to keep unobstructed blood and improve microcirculation to ischemic heart; can the generation of preventing cancer and development; there is atherosclerosis and coronary heart disease; immune system activity in ischemic heart disease, senile dementia, viral hepatitis, stomach ulcer and lifting wound treatment, and the effect of Tumor suppression.
The preparation of current trans-resveratrol is divided into chemical synthesis, culture plant cell, microwave extraction, the large class of ultrasonic extraction and solvent-extraction process etc. five; Chemical synthesis and culture plant cell method processing condition are harsh, complicated, and yield is low, is difficult to industrializing implementation; Though supersonic method and microwave method have the effect of increase yield but in this process, the singularity due to product very easily becomes article of manufacture to be oxidized, and is not suitable for, is also difficult to carry out, the most widely used or plant extraction process.
Apply to now production method and be mainly divided into two kinds of techniques; One is ethanol-extracted, then extraction into ethyl acetate, then strips with alcohol, and filtering and concentrating, drying obtains product.Another kind directly extracts by ethyl acetate, and then alcohol is stripped, and filtering and concentrating, drying obtains product.All there is the shortcoming that man-hour is long, equipment used is more, solvent loss is large, yield is not high, production consumes greatly, high in cost of production is common in these existing technology; The above method of what is more important cannot to be got rid of in (prevention) leaching process because being heated fully, make to remain in the zymin accelerate decomposition in the middle of raw material cause yield low loss.
Three, summary of the invention
The object of this invention is to provide a kind of method extracting resveratrol ingredient from giant knotweed, it uses single-solvent extraction, and technique is simple, and efficiently, low cost, Production Flow Chart is short, the production method that yield is high.
In order to realize object of the present invention, the present invention implements by the following technical solutions:
(1), by the starting material good through enzymolysis processing add the superoxide-dismutase that raw material weighs 1 ‰, the alcohol solvent adding 5 times of weight 80% concentration extracts, and its temperature controls at 45-65 DEG C of degree, each 2 hours, extracts 4 times altogether;
(2) after, extracting solution obtained above being merged, temperature controls below 55--60 DEG C, carry out vacuum concentration and reclaim ethanol completely, the ratio that concentrated solution weighs 5% according to raw material adds chitosan saturated solution, leave standstill 8--12 hour, extract is separated out in the mode of precipitation at normal temperatures, filters after precipitation completely, intercepts solid precipitation part;
(3), in solid sediment, the alcoholic degree adding 20 times of precipitate weight is the alcohol solvent of 40--45%, precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled under 55--60 DEG C of vacuum state, be concentrated into without after alcohol component, add the chitosan saturated solution weighing 5% ratio in raw material, under normal temperature, leave standstill 8--12 hour, centrifugation obtains the precipitate of solid;
(4) alcoholic degree, again adding 20 times of precipitate weight is the alcohol solvent of 40--45%, precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled under heating 55--60 DEG C of vacuum state, be concentrated into without after alcohol component, add the chitosan saturated solution that raw material weighs 5% ratio, under normal temperature, leave standstill 8--12 hour, centrifugation obtains the precipitate of solid, to obtaining the precipitate pure water washing of solid to washings non-pigment composition state;
(5) precipitate, after washing pulverizes the product both obtaining 50%-65% after vacuum-drying.
A kind of described method extracting resveratrol ingredient from giant knotweed, interpolation raw material weighs in the superoxide-dismutase prevention production process of 1 ‰ being present in material plant to lose activity for the enzyme decomposing polidatin and the decomposition of excessive enzyme no longer occurs; Thus protect the loss of resveratrol ingredient in leaching process
A kind of described method extracting resveratrol ingredient from giant knotweed, adopts the chitosan saturated solution of 5% to guide the precipitation of product in concentrated solution fast.
A kind of method extracting resveratrol ingredient from giant knotweed of the present invention, it amplifies actual measurement by technique; One, with the addition of in extraction process and can suppress to continue the de-enzyme agent ' superoxide-dismutase ' of enzyme digestion reaction and be present in material plant to lose activity for the enzyme decomposing polidatin in leaching process and excessive enzyme no longer occurs decompose; Thus protect the more existing industry of the loss of resveratrol ingredient (enterprise) in leaching process and can improve yield more than 30%; Reduce the content because of the harmful free radicals of enzymolysis generation in product simultaneously; The trans-resveratrol two, adopting the alcohol solvent of 40% content to coordinate chitosan solution to accelerate to be transferred in aqueous phase solution by solvent item is also separated out by precipitation in turbid solution fast completely with solid form.The product of the precipitation naturally link changing 2-4 days in traditional technology mode is complete in 12 hours; Three, in product emodin content less than 0.7% well below the company standard of industry 2.8%; Anthraquinone foreign matter content is less than 1/10 of traditional technology.
The present invention adds superoxide-dismutase that raw material weighs 1 ‰ and stops and the loss protecting the excessive decomposition in leaching process to cause and reduce the content of the harmful free radicals produced because of enzymolysis in product; The chitosan saturated solution of interpolation 5% is adopted to guide concentrated solution to separate out fast.Superoxide-dismutase and chitosan all do not add containing toxic component can not cause unnecessary injury in process.
In the present invention refer to giant knotweed containing resveratrol ingredient, peanut rhizome, the branches and leaves of grape, the plants such as mulberry leaf, as raw material, refer in particular to giant knotweed; The present invention by the superoxide-dismutase that adds of raw material anharmonic ratio example be form not under dissolved state, chitosan refers to and is being dissolved in the saturated solution in water.Due to industry product purity normally 50% content specification be not very high, comprise account for product half soluble impurity therefore technique adopt and add chitosan solution and accelerate art production process as the precipitation agent guided and corresponding shortening man-hour.
A kind of method extracting resveratrol ingredient from giant knotweed provided by the invention, it can improve yield more than 30% compared with existing production method.
Five, embodiment
Do carefully to describe furtherly to the present invention below in conjunction with embodiment.
The processing step that the present invention adopts optimizes gained by parallel test, and adopt vertical mode of amplifying to implement;
Embodiment 1:
To learn from else's experience warp after enzymolysis---detect Resveratrol content be 1.4% giant knotweed raw material 1 kilogram (eliminating water ratio) add 1 gram of superoxide-dismutase and add 5 liter of 80% concentration ethanol solvent simultaneously, heating and temperature control was 50 DEG C of refluxing extraction 2 hours, after filtering out extracting solution, add the extraction using alcohol 2 hours of 5 liters again, 4 times like this, the extracting solution obtained each batch merges control temperature and carries out vacuum concentration recovery ethanol at 60 DEG C, the ratio that extracting solution after concentrated weighs 5% in raw material adds chitosan saturated solution, leave standstill and separate out at normal temperatures for 10 hours, filter after precipitation completely,
Intercept solid precipitation part add 20 times of mass concentrations to precipitate be 40% alcohol solvent redissolve is carried out to the precipitate obtained and filters, insolubles discards, filtered liquid heating and temperature control 60 DEG C of concentration in vacuo, to without the chitosan saturated solution adding raw material after alcohol component and weigh 2% ratio, leave standstill precipitation in 10 hours under normal temperature.Centrifugation obtains the precipitate of solid;
The alcoholic degree again adding 20 times of precipitate weight be 40% alcohol solvent precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled after without alcohol component, to add the chitosan saturated solution that raw material weighs 5% ratio at heating 60 DEG C of concentration in vacuo, under normal temperature, leave standstill 10 hours, the extract that centrifugation obtains solid is separated out.With pure water washing under washings non-pigment composition state.
Precipitate after washing pulverize after vacuum-drying 57% product 23 grams, yield 93.6%.
Embodiment 2:
The giant knotweed raw material 10 kilograms (eliminating water ratio) being 1.4% through detection Resveratrol content after getting fermentation adds 10 grams of superoxide-dismutases and adds 50 liter of 80% concentration ethanol solvent simultaneously, heating and temperature control was 50 DEG C of refluxing extraction 2 hours, after filtering out extracting solution, add the extraction using alcohol 2 hours of 5 liters again, 4 times like this, the extracting solution obtained each batch merges control temperature and carries out vacuum concentration recovery ethanol at 60 DEG C, the ratio that extracting solution after concentrated weighs 5% in raw material adds chitosan saturated solution, leave standstill and separate out at normal temperatures for 12 hours, filter after precipitation completely.
Intercept solid precipitation part add 20 times of mass concentrations to precipitate be 40% alcohol solvent redissolve is carried out to the precipitate obtained and filters, insolubles discards, filtered liquid heating and temperature control 60 DEG C of concentration in vacuo, to without the chitosan saturated solution adding raw material after alcohol component and weigh 2% ratio, leave standstill precipitation in 12 hours under normal temperature.Centrifugation obtains the precipitate of solid.
The alcoholic degree again adding 20 times of precipitate weight be 40% alcohol solvent precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled after without alcohol component, to add the chitosan saturated solution that raw material weighs 5% ratio at heating 60 DEG C of concentration in vacuo, under normal temperature, leave standstill 12 hours, the extract that centrifugation obtains solid is separated out.With pure water washing under washings non-pigment composition state.
Precipitate after washing pulverize after vacuum-drying 55% product 238 grams, yield 93.5%.
Embodiment 3:
The giant knotweed raw material 100 kilograms (eliminating water ratio) being 1.4% through detection Resveratrol content after getting fermentation adds 100 grams of superoxide-dismutases and adds 500 liter of 80% concentration ethanol solvent simultaneously, heating and temperature control was 50 DEG C of refluxing extraction 2 hours, after filtering out extracting solution, add the extraction using alcohol 2 hours of 5 liters again, 4 times like this, the extracting solution obtained each batch merges control temperature and carries out vacuum concentration recovery ethanol at 60 DEG C, the ratio that extracting solution after concentrated weighs 5% in raw material adds chitosan saturated solution, leave standstill and separate out at normal temperatures for 12 hours, filter after precipitation completely.
Intercept solid precipitation part add 20 times of mass concentrations to precipitate be 40% alcohol solvent redissolve is carried out to the precipitate obtained and filters, insolubles discards, filtered liquid heating and temperature control 60 DEG C of concentration in vacuo gather saturated sugar soln to without the shell adding raw material after alcohol component and weigh 2% ratio, leave standstill precipitation in 12 hours under normal temperature.Centrifugation obtains the precipitate of solid.
The alcoholic degree again adding 20 times of precipitate weight be 40% alcohol solvent precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled after without alcohol component, to add the chitosan saturated solution that raw material weighs 5% ratio at heating 60 DEG C of concentration in vacuo, under normal temperature, leave standstill 12 hours, the extract that centrifugation obtains solid is separated out.With pure water washing under washings non-pigment composition state.
Precipitate after washing pulverize after vacuum-drying 54% product 2.4 kilograms, yield 92.5%.
Embodiment 4:
The giant knotweed raw material 500 kilograms (eliminating water ratio) being 1.4% through detection Resveratrol content after getting fermentation adds 0.5 kilogram of superoxide-dismutase and adds 2500 liter of 80% concentration ethanol solvent simultaneously, heating and temperature control was 50 DEG C of refluxing extraction 2 hours, after filtering out extracting solution, add the extraction using alcohol 2 hours of 5 liters again, 4 times like this, the extracting solution obtained each batch merges control temperature and carries out vacuum concentration recovery ethanol at 60 DEG C, the ratio that extracting solution after concentrated weighs 5% in raw material adds chitosan saturated solution, leave standstill and separate out at normal temperatures for 12 hours, filter after precipitation completely.
Intercept solid precipitation part add 20 times of mass concentrations to precipitate be 40% alcohol solvent redissolve is carried out to the precipitate obtained and filters, insolubles discards, filtered liquid heating and temperature control 60 DEG C of concentration in vacuo, to without the chitosan solution adding raw material after alcohol component and weigh 2% ratio, leave standstill precipitation in 12 hours under normal temperature.Centrifugation obtains the precipitate of solid.
The alcoholic degree again adding 20 times of precipitate weight be 40% alcohol solvent precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled after without alcohol component, to add the chitosan saturated solution that raw material weighs 5% ratio at heating 60 DEG C of concentration in vacuo, under normal temperature, leave standstill 12 hours, the extract that centrifugation obtains solid is separated out.With pure water washing under washings non-pigment composition state.
Precipitate after washing pulverize after vacuum-drying 55% product 11.5 kilograms, yield 90.4%.
Claims (1)
1. from giant knotweed, extract a method for resveratrol ingredient, it is characterized in that:
(1), by through the good starting material of enzymolysis processing, the alcohol solvent adding 5 times of weight 80% concentration extracts, and its temperature controls at 45-65 DEG C of degree, each 2 hours, extracts 4 times altogether;
(2) after, extracting solution obtained above being merged, temperature controls below 60 DEG C, carry out vacuum concentration and reclaim ethanol completely, the ratio that concentrated solution weighs 5% according to raw material adds chitosan saturated solution, leave standstill 12 hours, extract is separated out in the mode of precipitation at normal temperatures, filters after precipitation completely, intercepts solid precipitation part;
(3), in solid sediment, the alcoholic degree adding 20 times of precipitate weight is the alcohol solvent of 40%, precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled under 60 DEG C of vacuum states, be concentrated into without after alcohol component, add the chitosan saturated solution weighing 5% ratio in raw material, under normal temperature, leave standstill 12 hours, centrifugation obtains the precipitate of solid;
(4) alcoholic degree, again adding 20 times of precipitate weight is the alcohol solvent of 40%, precipitate is dissolved and filter, insolubles discards, then filtered liquid temperature is controlled under heating 60 DEG C of vacuum states, be concentrated into without after alcohol component, add the chitosan saturated solution that raw material weighs 5% ratio, under normal temperature, leave standstill 12 hours, centrifugation obtains the precipitate of solid, to obtaining the precipitate pure water washing of solid to washings non-pigment composition state;
(5) precipitate, after washing pulverizes the product both obtaining 50%-65% after vacuum-drying.
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| An Antiinflammatory and Reactive Oxygen Species An Antiinflammatory and Reactive Oxygen Species Cuspidatum Containing Resveratrol;Husam Ghanim等;《J Clin Endocrinol Metab》;20100609;第95卷(第9期);第E1-E8页 * |
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